反应详情

温度

-10 °C

4-Methoxyacetophenone (1.4 g) and sodium hydroxide (0.2 g) were suspended in 15 Ml of methanol pre-chilled at −10° C. The solution was kept for 1 hr under 0° C. with stirring. Benzaldehyde (1 g) was added thereto, and refluxed for 10 hr at room temperature with stirring. After neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate. The extracted organic phase was dried with anhydrous magnesium sulfate, and evaporated under vacuum. The resulting 1.3 g of white powder was purified through silica gel column chromatography (5×3 cm, Merk), which is eluted with n-hexane:ethylacetate (v/v, 1:7). The purified compound was identified as follows:

1. temperaturerefluxed for 10 hr at room temperature
2. stirringwith stirring
3. extractionAfter neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate
4. dry with materialThe extracted organic phase was dried with anhydrous magnesium sulfate
5. customevaporated under vacuum
6. customThe resulting 1.3 g of white powder was purified through silica gel column chromatography (5×3 cm, Merk), which
7. washis eluted with n-hexane